超高效液相色谱–串联质谱法同时检测蔬菜中17种氨基甲酸酯类农药残留
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摘要
建立用超高效液相色谱–串联质谱仪对蔬菜中17种氨基甲酸酯类农药残留同时检测的方法。对传统的Qu ECh ERS前处理方法进行优化和改良,将样品置于萃取管中,加入乙腈溶液提取,振荡离心后,将上清液移入净化管中净化,用超高效液相色谱–串联质谱仪进行检测。17种待测农药的质量浓度在5~500 ng/mL范围内与其色谱峰面积线性关系良好,相关系数(r)大于0.99,检出限为0.3~1.6μg/kg。在5,10,50μg/kg 3个浓度水平进行添加回收试验,平均回收率在61.0%~107.6%之间,测定结果的相对标准偏差为1.6%~17.6%(n=6)。该方法检测时间较短,检出限低,测量重现性高,适用于蔬菜中17种氨基甲酸酯类农药残留的同时检测。
A method for determination of 17 kinds of carbamate pesticides residue in vegetables by UPLC–MS/MS was established. The traditional pretreatment method of Qu ECh ERS was optimized and improved,in the extraction tube,the sample was extracted by the acetonitrile solution,and after the shock centrifugation,the upper cleaning liquid was transferred into the purifying tube to purify,and then detected by UPLC–MS/MS. The mass concentration of 17 kinds of pesticides had good relationship with its chromatographic peak area between 5–500 ng/mL, and the correlation coefficient(r) was more than 0.99,the detection limits were 0.3–1.6 μg/kg. At the level of 5,10,50 μg/kg 3 concentration level,the average recovery rate was 61.0%–107.6%,and the relative standard deviation of determination results was 1.6%–17.6%(n=6). This method is suitable for the detection of 17 kinds of carbamate pesticide residues in vegetables with short detection time, low detection limit and high reproducibility.
A method for determination of 17 kinds of carbamate pesticides residue in vegetables by UPLC–MS/MS was established. The traditional pretreatment method of Qu ECh ERS was optimized and improved,in the extraction tube,the sample was extracted by the acetonitrile solution,and after the shock centrifugation,the upper cleaning liquid was transferred into the purifying tube to purify,and then detected by UPLC–MS/MS. The mass concentration of 17 kinds of pesticides had good relationship with its chromatographic peak area between 5–500 ng/mL, and the correlation coefficient(r) was more than 0.99,the detection limits were 0.3–1.6 μg/kg. At the level of 5,10,50 μg/kg 3 concentration level,the average recovery rate was 61.0%–107.6%,and the relative standard deviation of determination results was 1.6%–17.6%(n=6). This method is suitable for the detection of 17 kinds of carbamate pesticide residues in vegetables with short detection time, low detection limit and high reproducibility.
引文
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[11]陈晓水,边照阳,唐纲岭,等.气相色谱–串联质谱技术分析烟草中的132种农药残留[J].色谱,2012,30(10):1 043–1 055.
[12]孙欣,齐莉,秦廷亭,等.Qu ECh ERS–气相色谱–三重四极杆质谱法检测黄瓜中的19种邻苯二甲酸酯[J].色谱,2014,32(11):1 260–1 265.
[13]吴岩,姜冰,徐义刚,等.Qu ECh ERS–液相色谱–串联质谱法同时测定果蔬中16种农药残留[J].色谱,2015(3):228–234.
[14]林涛,邵金良,刘兴勇,等.Qu ECh ERS–超高效液相色谱–串联质谱法测定蔬菜中41种农药残留[J].色谱,2015(3):235–241.
[15]高阳,徐应明,孙扬,等.Qu ECh ERS提取法在农产品农药残留检测中的应用进展[J].农业资源与环境学报,2014(2):110–117.
[2]孙丽娜,付良月,高朋.蔬菜农药残留对人体危害及预防措施[J].科技与企业,2014(16):425.
[3]刘嫦娥,胡波,吴敏,等.农产品农药残留的危害与预防[J].现代农业科技,2012(14):290.
[4]何佩雯,赵海誉,杜钢,等.气相色谱技术在中药农药残留检测中的应用[J].中国实验方剂学杂志,2010,16(2):126–134.
[5]廖和菁,张雪春,胡礼渊,等.气相色谱法同时测定茶叶中10种有机磷农药残留[J].中国食品卫生杂志,2015,27(1):41–44.
[6]钱莹,苏小川.气相色谱法在有机磷农药残留量分析中的应用与进展[J].广西科学院学报,1997(2):23–28.
[7]董振霖,杨春光,肖珊珊,等.气相色谱和气相色谱–质谱法测定食品中乙草胺残留[J].分析化学,2009,37(5):698–702.
[8]李晓颍,张红医,常巧英,等.气相色谱–四极杆飞行时间质谱准确鉴定常见水果蔬菜中的农药残留[J].色谱,2014,32(3):268–277.
[9]施家威,李继革,王玉飞,等.分散固相萃取–气相色谱–三重四极杆质谱分析蔬菜中112种农药残留[J].色谱,2012,30(6):602–612.
[10]马智玲,赵文,李凌云,等.气相色谱–三重四极杆串联质谱法快速测定蔬菜水果中129种农药的残留量[J].色谱,2013,31(3):228–239.
[11]陈晓水,边照阳,唐纲岭,等.气相色谱–串联质谱技术分析烟草中的132种农药残留[J].色谱,2012,30(10):1 043–1 055.
[12]孙欣,齐莉,秦廷亭,等.Qu ECh ERS–气相色谱–三重四极杆质谱法检测黄瓜中的19种邻苯二甲酸酯[J].色谱,2014,32(11):1 260–1 265.
[13]吴岩,姜冰,徐义刚,等.Qu ECh ERS–液相色谱–串联质谱法同时测定果蔬中16种农药残留[J].色谱,2015(3):228–234.
[14]林涛,邵金良,刘兴勇,等.Qu ECh ERS–超高效液相色谱–串联质谱法测定蔬菜中41种农药残留[J].色谱,2015(3):235–241.
[15]高阳,徐应明,孙扬,等.Qu ECh ERS提取法在农产品农药残留检测中的应用进展[J].农业资源与环境学报,2014(2):110–117.